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Bongkrekic acid high-selectivity enrichment solid-phase micro-extraction probe as well as preparation method and application thereof

A rice yeast acid, high-selectivity technology, applied in the field of analysis and testing, can solve the problems of long chromatographic separation time, a large number of organic solvents, cumbersome and other problems, and achieve the effects of low price, high selective adsorption capacity, and simple production.

Active Publication Date: 2021-11-30
INST OF ANALYSIS GUANGDONG ACAD OF SCI (CHINA NAT ANALYTICAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nevertheless, HPLC and HPLC-MS methods require complex and tedious sample preparation, use of large amounts of organic solvents, and long chromatographic separation times

Method used

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  • Bongkrekic acid high-selectivity enrichment solid-phase micro-extraction probe as well as preparation method and application thereof
  • Bongkrekic acid high-selectivity enrichment solid-phase micro-extraction probe as well as preparation method and application thereof
  • Bongkrekic acid high-selectivity enrichment solid-phase micro-extraction probe as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A high-selectivity enrichment solid-phase microextraction probe of rice yeast acid, its preparation method is as follows:

[0040] (1) Preparation of solid substrate: Provide a wooden stick with a length of 2 cm and a tip diameter of 0.05 to 0.20 mm, soak the wooden stick in methanol for 10 minutes, then clean it with deionized water, and dry it naturally to obtain a solid-phase microstructure. the solid matrix of the extraction probe;

[0041] (2) Surface modification of solid substrate: Dissolve 1mL of γ-methacryloxypropyltrimethoxysilane in 20mL of anhydrous toluene, add the solid substrate obtained in step (1), blow in nitrogen, and heat to 110°C React for 12 hours. After the reaction is completed, wash the solid substrate three times with absolute ethanol, and dry it naturally to obtain a surface-modified solid substrate;

[0042] (3) Molecularly imprinted polymerization reaction: Add 10mL chloroform and 20mL acetonitrile into a 100mL round bottom bottle to form a...

Embodiment 2

[0045] A kind of solid-phase microextraction and the method for detection of oryzae acid by atmospheric pressure open mass spectrometry, it comprises the following steps:

[0046] Solid-phase microextraction: The extraction method of the sample is consistent with the conventional solid-phase microextraction method, and the direct extraction mode is adopted. Before extraction, the solid-phase microextraction probe prepared in Example 1 was rinsed with methanol for 30 s. After the extraction, the solid-phase microextraction probe was quickly taken out from the sample, washed in pure water for 10 seconds, and then taken out. After being dried naturally, the probe was analyzed by atmospheric pressure open electrospray mass spectrometry.

[0047] Atmospheric pressure open mass spectrometry: fix the extracted solid-phase microextraction probe on a three-dimensional mobile stage, align the tip of the probe with the entrance of the mass spectrometer and be 10 mm away from the entrance...

Embodiment 3

[0050] Put the solid-phase microextraction probe prepared in Example 1 into 100 mL of the spiked water sample containing oryzae acid at a concentration of 10 ng / mL, and extract for 10 min under stirring at 800 rpm. After the extraction was completed, the solid-phase microextraction probe was taken out from the sample, washed in pure water for 10 s, and then subjected to natural pressure open electrospray mass spectrometry analysis according to the method of Example 2 after being dried naturally. Figure 5 After the solid-phase microextraction probe prepared for Example 1 extracted oryzanic acid (10 μg / L) in the water sample, the mass spectrogram was obtained by performing atmospheric pressure open electrospray mass spectrometry analysis. From Figure 5 It can be seen from the analysis results that the solid-phase microextraction probe of the present invention has a very excellent enrichment ability for oryzanic acid in food, and the enrichment ability is as high as thousands o...

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Abstract

The invention discloses a preparation method of a bongkrekic acid high-selectivity enrichment solid-phase micro-extraction probe. The preparation method comprises the following steps of: providing a solid substrate; carrying out surface modification on the solid substrate to enable the surface of the solid substrate to be rich in methacryloyloxy so as to obtain a surface modified solid substrate; and carrying out a molecular imprinting polymerization reaction on the surface modified solid substrate through a molecular imprinting technology by taking methacryloyloxyethyl trimethyl ammonium chloride and octadecyl methacrylate as functional monomers and vitamin A acid and (R)-12-hydroxy-cis-9-octadecenoic acid as template molecules to enable a molecularly imprinted coating with high selective adsorption capacity on bongkrekic acid to be attached to the surface of the solid substrate. The solid-phase micro-extraction probe disclosed by the invention can be used for efficiently extracting and enriching bongkrekic acid in complex food, the enrichment coefficient can reach thousands of times, and the detection limit can reach the level of [mu]g / L. The probe is simple to manufacture, low in price, disposable, capable of effectively preventing cross contamination and memory effect, and especially suitable for rapid analysis and detection of food safety.

Description

technical field [0001] The invention belongs to the technical field of analysis and testing, and in particular relates to a solid-phase microextraction probe for highly selective enrichment of rice yeast acid and its preparation method and application. Background technique [0002] Bongkrekic acid (BA) is a long-chain fatty acid biotoxin produced by Pseudomonas coconut (Burkholderiagladioli pathovar Cocovenenans), which can inhibit the adenine nucleotide translocation enzyme ( ANT) activity, leading to the damage of brain, heart, liver, kidney and other organs, oral half lethal dose (LD) of mice 50 ) is 3.16 mg / kg. The structure of rice yeast acid is stable, and it is difficult to remove it during conventional food processing. Human consumption of food contaminated by rice yeast acid can cause nausea, vomiting, and lack of energy. Ingestion of 1-1.5mg can even lead to death. Pseudomonas cocos is a common food-borne pathogen in the environment. Foods such as grains, ferment...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30C08F220/34C08F220/18G01N27/62
CPCB01J20/268B01J20/28042C08F220/34C08F220/1818G01N27/62
Inventor 杨运云钟淳菲陈啸天方舒婷侯雅君
Owner INST OF ANALYSIS GUANGDONG ACAD OF SCI (CHINA NAT ANALYTICAL
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